Oxidized oil for artificial textile materials



May 26, 1936- G. wl SEYMOUR OXIDIZED OIL FOR ARTIFICIAL TEXTILE MATERIALS Filed June 29, 1934 INVENTOR. SEYMOUR Patented Ma 26, 1936 OHDIZED OIL FOR ARTIFICIAL TEXTILE MATERIALS George W. Seymour, Cumberland, Md., assignor to Celanese Corporationof America, a corporation of Delaware Application June 29, 1934, Serial No. 732,992

I '2 Claims. (01.87-12) This invention relates to the method and device for oxidizing vegetable oils for the use in. manufacturing artificial filaments. This inven- I tion further relates to the specific method of oxidizing vegetable oils to produce a product of low viscosity and low surface tension. An object of the invention is the simple and inexpensive 'method and device for oxidizing vegetable oils. Another object of the invention is the production of an oxidized oil of low acidity,

low viscosity and low surface tension. Other objects of the invention will appear from the following detailed description. In the drawing is shown a side elevation partially in section of a device for, oxidizing oils.

According to my invention I have developed an apparatus and method for oxidizing vegetable oils, specifically to be used for incorporation with yarns and films of organic derivatives of cellulose. The apparatus and method of my invention is economical, efiicient, and productive of anoxidized oil', having enhanced properties for textile purposes which oxidized oils may be employed in amounts of from 1 to on the weight of the 25 cellulose derivative in filaments and foils formed of derivatives of cellulose.

The oils produced by this invention are applicable to filaments, yarns, films and foils containing organic derivatives of cellulose such as the organic esters of cellulose and the cellulose ethers.

Examples of organic esters of cellulose are cellulose acetate, cellulose propionate, cellulose butyrate and cellulose formate while examples of .cellulose ethers are methyl cellulose, ethyl cellulose and benzyl cellulose. The oils produced by this invention are also applicable to uses wherever oxidized oils of low viscosity and low surface tension are desired.

Filaments and films may be formed from organic derivatives of cellulose by dissolving the same in suitable solvents and extruding the solution through suitable orifices or casting or flowing the solution onto suitable surfaces in a solidifying medium. For the purpose of this invention this solution will be termed the spinning solution whether for spinning filaments or forming films or foils. In employing organic esters of cellulose it is quite common to employ acetone or mixtures of acetone and water or alcohol as the solvent in the spirming solution. This solvent may be removed from the formed or shaped article by evaporation as in dry spinning and wheelcasting or the cellulosic material may be precipitated from the solvent by liquids as in wet methods of spinning.

By any method of forming the articles it. is often necessary that the spimiing solution be kept for hours prior to being formed into articles. Due to this standing, efiect materials added to the spinning solution and thus incorporated with the article, must be such that they do not readily separate out in the solution or as it is termed, form an unstable solution. One of the advantages of this invention is that a lubricated and pliable filament and/ or foil is produced containing an oil which is somewhat soluble in acetone and acetone mixtures. Moreover, the spinning solution acquires long stability due to the presence of the oil.

Some oils upon oxidation become very viscous which prohibits their use as a yarn lubricant while others, such as cocoanut oil, corn oil etc., develop a high acidity during oxidation which renders them less suitable for the purpose of this invention. I have found, however, that oxidized olive oil, peanut oil, cottonseed oil, castor oil or other,like vegetable oil have a great compatibility with organic derivatives of cellulose in acetone or acetone mixture solutions. These oxidized oils are also soluble in'acetone solutions to the extent of more than 3%. Thus when they are mixed into spinning solutions they are compatible therewith and form'relatively stable spinning mixtures. These oxidized oils may be used in amounts of from 1 to 25% on the weight of the organic derivative of cellulose.

The oxidation of the oil is preferably carried out under conditions that do not promote polymerization and other special conditions which form a part of my invention, although normally blown oil may be employed. It is obvious that best operating results are obtained with the lower viscosity and lower surface tension products. The temperature and pressure under, which the reaction can be carried out vary inan inverse ratio, that is, when the pressure is increased the temperature might well be decreased, however, I have found that oils oxidized under greater pressure and lower temperatures produce a type of lubricant most suitable for the purpose of incorporating in filaments and films i. e. those that are most free of acid and have low viscosity and low surface tension.

In the drawing is shown a device for expeditiously oxidizing oils to produce oxidized oils that are especially suitable for employment as a yarn lubricant and textile aids when incorporated with filaments and films of organic derivatives .of cellulose. In the drawing I is a kettle sealed against the atmosphere and capable of withstanding high pressure from the inside. This kettle may be equipped with a steam jacket 2 supplied with wet or dry steam of any suitable pressure by means of the openings 3 and 4 and the header 5 connected to a suitable source of steam by the 5 pipe line 6. The condensate may be withdrawn through the pipe line I through a steam trap 8 and condensate line 9. Any other heating means such as an open flame, electric resistance or conductance may be employed in place of the steam jacket.

The kettle is equipped with suitable sealing flanges l0 that .may be held in sealed position by any suitable means such as clamps or bolts and any suitable type of gaskets or cement may be employed between the flanges.

In the bottom of the kettle I there is a trap II from which leads a drain pipe line [2 having a valve l3 for withdrawing the liquid contents of the kettle. In the drain pipe line l2 there may be a dirt pocket 36 and means for draining the kettle. Between the bottom of the kettle and the valve l3 in the pipe line I2 is a side pipe line H containing a filter IS. The, pipe line [4 is connected through a valved line [6 and also through a pump H to a pipe line l8 entering the kettle from the top. The pump I I may be driven by any suitable power means such as an electric motor I9; The feed pipe line l8 at a point in the top of the kettle is equipped with a header 20 that contains a series of spray nozzles 2|. The upper end of the pipe line I8 isconnected to a suitable gauge 22 protected with a valve 23. This circuit is adapted to draw liquids from the bottom of the kettle and eject them in atomized or flnely divided spray form into the gaseous space at the top of the kettle.

From a suitable source .of oxygen, such as tank 24, a, pipe line 25 leads through a regulating valve 26 and is equipped with suitable pressure gauges 21 and 28 on either side of the regulating valve. The pipe line 25 is connected into a header 29 which in turn is connected to a pop-off safety valve 30, a vent 3|, a pressure gauge 32 and to the kettle at 33. By this means a regulated pressure and quantity of oxygen may be admitted or supplied to the kettle. The gas need not be pure oxygen but merely a gas of high oxygen content such as a mixture of air and'oxygen.

A well 34 is provided for ascertaining the temperature, by any suitable means, of the working zones in the kettle. -A tap 35 is provided for periodically taking samples of the circulating liquid.

In operation the kettle l is filled to about the height of the water jacket 2 with the oil to be oxidized, say olive oil and a catalyst, say 3.5 to 4.5% preferably 4% of whale oil, which percentage gives consistent results, that is, it has the minimum amount of separation with the maximum speed of catalytic reaction.

The pressure of the oxygen may be any suitable pressure dependent upon the. temperature employed. .It is preferable however to employ pressures of above 45 lbs. per square inch, say between 45 and 60 lbs. per square inch above atmospheric pressure. The higher pressures and lower temperatures result in an oxidized oil of lower viscosity that more readily distributes itself in and on the yarn. The temperature may be any suitable temperature from 100 C. to 200 C. but preferably from 100 C. to 125 C.

The rate of flow of the oil through the spray nozzles may be any suitable rate and the header 20 may be equipped with 1 to 12 nozzles with a 75 pump pressure of between and 20 1bs. per

square inch. A large variation in the rate of recirculation of the oil is permissible without a great eifect upon the quantity of oil oxidized per unit time or the type of oil produced.

As description and not as a limitation the fol- 5 lowing example is given.

E zample 30 gallons of raw olive oil containing 4% whale oil is introduced into the apparatus. The header 20-is equipped with 6 nozzles and a pump pressure of 15 lbs. per square inch maintained for 44 hours. The temperature of the oil in the kettle is maintained during this time at 120 C. and a kettle pressure of 48-50 lbs. per inch is maintained. The oxidized oil produced is light in color and has a viscosity at 210 F. of 150 Saybolt seconds or less with a water tolerance of 8.5%. Other desirable oils give similar viscosities say from 140 to 175 at 210 F. and water tolerances from 5 to 10%. By water tolerance is meant the amount of a mixture .of 70 parts diethylene glycol to 30 parts of water, soluble in or absorbed by the oil. The oil is not actually hydroscopic, but with the accompanying diethylene glycol it will tolerate a relatively high percent of water.

To a solution containing 1 part cellulose acetate dissolved in 3 parts by weight of acetone, there is added about 0.10 part by weight of this oxidized oil, to form a spinning solution. This solution is spun by the drymethod of spinning. The filaments produced are pliable and may be knit into fabrics with a free delivery. The yarns formed from a group of filaments may be further lubricated by applying to same a coating of a mixture of oxidized oil,water and glycol or a derivative or substitution product of glycol.

It-is to be understood that the foregoing detailed description is merely given by way of illustration and many alterations may be made therein without departing from the spirit of my invention.

Having described my invention what I desire to secure by Letters Patent is:

1. A method of oxidizing vegetable oils, which comprises subjecting vegetable oil to the action of oxygen at a temperature between and 200 C. and a pressure of 45 to 60 lbs. per square inch. in the presence of a small amount of whale oil.

2. A method of oxidizing vegetable oils, which 60 comprises subjecting vegetable oil in the form of a spray to the action of oxygen at a temperature between 100 and 200 C. and a pressure of 45 to 60 lbs. per square inch, in the presence of a small amount of whale oil.

3. A method of oxidizing vegetable oils, which comprises subjecting vegetable oil to the action of oxygen at a temperature between 100 and 200 C. and a pressure of 45 to 60 lbs. per square inch, in the presence of whale oil in an amount 60 equal to from 3.5 to 4.5% based on the weight of the oil being oxidized. I

4; Method of oxidizing vegetable oils, which comprises subjecting vegetable oil to the action of oxygen at a temperature of C. and a pres- 65 sure of 48 to 50 lbs. per square inch, in the presence of whale oil in an amount equal to 4% based on the weight of the oil being oxidized.

, 5. Method of oxidizing vegetable oils, which comprises spraying vegetable oil containing a 70 small amount of whale oil as catalyst into a stagnant atmosphere of a gas comprising oxygen at a temperature between 100 and 200 C. and a pressure of 45 to 60 lbs. per square inch.

6. Method of oxidizing vegetable oils. which 75 comprises spraying vegetable oil containing, as catalyst, whaleoil, in an amount equal to from 3.5 to 4.5% based on the weight of the oil to be oxidized, into a stagnant atmosphere of a gas comprising oxygen at a temperature between 100 and 200 C. and a pressure of 45 to 60 lbs. per square inch.

7. Method of oxidizing vegetable oils. which comprises spraying vegetable oil containing, as catalyst, whale oil in an amount equal to 4% based onthe weight of the oil to be oxidized, into a stagnant atmosphere of a gas comprising oxygen at a temperature of 120 C. and a pressure of 5 48 to 50 lbs. per square inch.

GEORGE w. smoun. 

